Gas-solid reaction apparatus and gas-solid reaction method

Abstract

The application provides a gas-solid reaction device and a gas-solid reaction method, relates to the technical field of reaction equipment, and comprises a riser reaction assembly, a down-flow bed reaction assembly and a separation circulation assembly. The riser reaction assembly comprises a pre-reaction section and a riser section. The down-flow bed reaction assembly comprises a down-flow bed which is in communication with the riser. The separation circulation assembly comprises an axial-flow gas-solid separator, a storage bed and a connecting pipeline. The inlet of the axial-flow gas-solid separator is in communication with the outlet of the down-flow bed. The gas phase outlet of the axial-flow gas-solid separator is in communication with the gas phase zone of the storage bed. The solid phase outlet of the axial-flow gas-solid separator is in communication with the storage zone of the storage bed. The riser reaction assembly and the down-flow bed reaction assembly are arranged, so that the gas-solid reaction of superfine particles mainly occurs in the dilute phase bed section. The contact and mixing efficiency between the gas and the solid are effectively enhanced, and problems such as insufficient gas-solid contact, adhesion between particles and heat exchange dead zones in the dense phase bed section are avoided.

Description

Technical Field

[0001] The present invention relates to the technical field of reaction equipment, and in particular to a gas-solid reaction device and a gas-solid reaction method. Background Art

[0002] Geldart C particles, also known as ultrafine particles, typically have a particle size less than 20 μm. Due to the strong van der Waals and electrostatic forces between ultrafine particles, agglomeration, channeling, and slugging are common during the fluidization process, severely impacting the stability of the fluidized bed operation and thus limiting the application of ultrafine particles in fluidized beds. However, with the continuous development of fields such as petroleum refining, chemical engineering, and material preparation, improving the fluidization state of ultrafine particles and applying them to the preparation of chemical products has become increasingly important. Chemical vapor deposition (CVD) is a typical powder reaction and preparation technology, widely used in the preparation of materials such as photovoltaic polysilicon, carbon silicon anodes, and silicon carbide. However, existing CVD applications commonly suffer from several issues, such as wall adhesion of the feed gas within the reactor, the presence of heat exchange dead zones within the reactor, and adhesion between deposited particles. Fluidized bed reactors offer many advantages, including high mass and heat transfer efficiency, uniform internal temperature distribution, vigorous gas-solid mixing, and wide operational flexibility. In recent years, the industry has combined fluidization technology with chemical vapor deposition and gradually applied it to existing chemical vapor deposition processes in an attempt to solve the above problems.

[0003] For example, Chinese patent document CN1198962A discloses a fluidized bed reactor for gas-solid phase processing of ultrafine particles. While this improves the problem of agglomeration of ultrafine particles during flow to some extent, the presence of a large number of internal components significantly increases the risk of wall adhesion reactions, and there is a lack of specific implementation measures for gas-solid separation in the downstream production process. Chinese invention patent CN114850283B discloses a fluidized reaction system with surface coating of ultrafine particles. In this patent document, the deposition carrier and deposition feed gas still exist in a dense phase bed in areas such as the bottom of the product tank. In this case, even with the installation of mechanical stirring paddles, it is still difficult to avoid problems such as inter-particle adhesion and uneven temperature distribution in this area. At the same time, the gas-solid flow in the riser is generally a ring-core structure, and the traditional bottom feeding method will aggravate the problem of particle adhesion at the side walls of the riser. In addition, the traditional cyclone separator has a low separation efficiency for ultrafine particles, and the use of a traditional cyclone separator coupled with a filter for dust removal will significantly reduce the stable operation time of the entire device. Chinese patent document CN117721434A discloses a reactor and method for vapor deposition of ultrafine particles. This patent improves the fluidized bed in the main reaction zone from a dense phase to a dilute phase, effectively enhancing gas-solid mixing within this zone and improving inter-particle adhesion. However, the ultra-short, rapid gas-solid separation structure has relatively low sizing efficiency for ultrafine particles, and the patent also lacks further treatment measures for residual particles. Therefore, technical issues such as low gas-solid mixing efficiency, numerous dead zones in the reaction, and difficulty in subsequent separation, which urgently need to be addressed in existing processes, are currently under investigation. Summary of the Invention

[0004] In order to overcome the above-mentioned defects of the prior art, the technical problem to be solved by the embodiments of the present invention is to provide a gas-solid reaction device and a gas-solid reaction method for solving at least one of the above-mentioned technical problems.

[0005] The above-mentioned object of the present invention can be achieved by adopting the following technical solutions. The present invention provides a gas-solid reaction device, comprising:

[0006] A riser reaction assembly, the riser reaction assembly comprising a pre-reaction section and a riser section connected to the outlet of the pre-reaction section;

[0007] A downer reaction assembly, the downer reaction assembly comprising a downer, the downer and the riser section being arranged side by side, the inlet of the downer and the outlet of the riser section being connected via an elbow;

[0008] A separation circulation assembly includes an axial flow gas-solid separator, a storage companion bed, and a connecting pipeline connecting the outlet of the storage companion bed and the inlet of the pre-reaction section. The connecting pipeline is provided with a fluidizing gas inlet. The inlet of the axial flow gas-solid separator is connected to the outlet of the descending bed. The gas phase outlet of the axial flow gas-solid separator is connected to the gas phase area of ​​the storage companion bed through a purified gas discharge pipe. The solid phase outlet of the axial flow gas-solid separator is connected to the storage area of ​​the storage companion bed through a captured particle discharge pipe.

[0009] In a preferred embodiment of the present invention, the radial dimension of the pre-reaction section is larger than the radial dimension of the lifting pipe section, and a first diameter reduction structure is provided between the pre-reaction section and the lifting pipe section; and / or, the radial dimension of the pre-reaction section is larger than the radial dimension of the connecting pipeline, and a first diameter expansion structure is provided between the pre-reaction section and the connecting pipeline; and / or, the radial dimension of the downer is larger than the radial dimension of the elbow, and a second diameter expansion structure is provided between the downer and the elbow; and / or, the radial dimension of the downer is larger than the radial dimension of the axial flow gas-solid separator, and a second diameter reduction structure is provided between the downer and the axial flow gas-solid separator.

[0010] In a preferred embodiment of the present invention, the gas-solid reaction device also includes at least one diffusion distributor arranged in the pre-reaction section, the outlet of the connecting pipeline is connected to the diffusion distributor, and the diffusion distributor includes an outlet surface provided with diffusion holes, and the porosity of the outlet surface is 5% to 50%.

[0011] In a preferred embodiment of the present invention, the gas-solid reaction device further comprises a first loop pipe distributor arranged in the pre-reaction section, the first loop pipe distributor being arranged horizontally and placed upstream of the diffusion distributor; and / or, the gas-solid reaction device further comprises a second loop pipe distributor arranged in the material storage companion bed, the second loop pipe distributor being arranged horizontally and placed at the bottom of the material storage companion bed.

[0012] In a preferred embodiment of the present invention, the ratio of the diameter of the pre-reaction section to the diameter of the riser section is 1.2 to 3; and / or the bending radius R of the elbow and the diameter of the elbow are 0.5 to 10; and / or the ratio of the diameter of the downer to the diameter of the pre-reaction section is 0.5 to 3.

[0013] In a preferred embodiment of the present invention, at least one row of first gas-phase feed hole groups are provided on the pre-reaction section along the circumference of the pre-reaction section; and / or, at least one row of second gas-phase feed hole groups are provided on the riser section along the circumference of the riser section; and / or, at least one row of third gas-phase feed hole groups are provided on the downer section along the circumference of the downer.

[0014] In a preferred embodiment of the present invention, the first gas-phase feed hole group includes at least one first gas-phase feed hole arranged on the pre-reaction section along the height direction, and a first gas-phase nozzle arranged on each of the first gas-phase feed holes, and the angle between the incident direction of the first gas-phase nozzle and the movement direction of the multiphase fluid in the pre-reaction section is 10° to 170°; and / or, the second gas-phase feed hole group includes at least one second gas-phase feed hole arranged on the riser section along the height direction, and a second gas-phase nozzle arranged on each of the second gas-phase feed holes, and the angle between the incident direction of the second gas-phase nozzle and the movement direction of the multiphase fluid in the riser section is 10° to 170°; and / or, the third gas-phase feed hole group includes at least one third gas-phase feed hole arranged on the down-bed along the height direction, and a third gas-phase nozzle arranged on each of the third gas-phase feed holes, and the angle between the incident direction of the third gas-phase nozzle and the movement direction of the multiphase fluid in the down-bed is 10° to 170°.

[0015] In a preferred embodiment of the present invention, the gas-solid reaction device further comprises a dust-containing gas filtering assembly disposed on top of the storage bed.

[0016] In a preferred embodiment of the present invention, the gas-solid reaction device further comprises a discharge valve arranged at the bottom of the material storage companion bed, and a discharge valve arranged at the outlet of the material storage companion bed.

[0017] The present invention also provides a gas-solid reaction method, which is implemented using the aforementioned gas-solid reaction device. The gas-solid reaction method comprises the following steps:

[0018] Close the discharge valve and open the gas phase supply of the second ring pipe distributor to make the ultrafine particles in the storage bed in a flowing state;

[0019] Open the discharge valve and the fluidizing gas inlet at the same time to introduce fluidizing gas and feed gas into the connecting pipeline to transport ultrafine particles, and maintain the superficial gas velocity in the riser reaction assembly within the entrained gas range;

[0020] Opening the first loop distributor to introduce supplementary fluidizing gas into the pre-reaction section to avoid formation of a dead zone at the bottom of the pre-reaction section;

[0021] During the reaction of the ultrafine particles, fluidizing gas and feed gas are introduced into the riser reaction assembly and / or the downer reaction assembly to maintain the feed gas concentration in the reaction assembly; wherein the feed gas injection velocity in the riser reaction assembly and / or the downer reaction assembly is 10 m / s to 100 m / s;

[0022] After the ultrafine particles have reacted in the riser reaction assembly and the downer reaction assembly in sequence, the multiphase fluid output from the downer is separated by an axial flow gas-solid separator, the separated ultrafine particles are transported back to the storage companion bed to continue circulating, and the separated gas phase fluid is transported back to the storage companion bed and discharged after being filtered.

[0023] When the ultrafine particles complete the reaction cycle, the discharge valve is closed to stop the cycle, and the discharge valve is opened to discharge the ultrafine particles.

[0024] The technical solution of the present invention has the following significant beneficial effects:

[0025] The gas-solid reaction device described in the present invention is suitable for ultrafine particles. By providing a riser reaction assembly and a downer reaction assembly, the gas-solid reaction of ultrafine particles occurs primarily in the dilute bed section, effectively enhancing the contact and mixing efficiency between the gas and the solid, and avoiding the common problems of insufficient gas-solid contact, interparticle adhesion, and heat exchange dead zones in the dense bed section. Furthermore, by expanding the diameter of the downer, not only is the agglomeration of ultrafine particles during flow significantly reduced, but the solid concentration within the downer is also moderately increased, further improving the gas-solid contact and mixing efficiency. Furthermore, an axial flow gas-solid separator is configured at the end of the downer, achieving rapid and efficient gas-solid separation, reducing the burden on subsequent filtration components, and optimizing the stable operating cycle of the entire device. By configuring the riser reaction assembly, downer reaction assembly, and separation circulation assembly to form a circulation pipeline, the total reaction time of the solid phase can be adjusted as needed, enhancing operational flexibility. The gas-solid reaction device also offers advantages such as space conservation and high operational flexibility, improving overall reaction efficiency and system reliability. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following briefly introduces the drawings required for use in the description of the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.

[0027] The drawings described herein are for illustrative purposes only and are not intended to limit the scope of the present invention in any way. In addition, the shapes and proportional dimensions of the various components in the drawings are merely illustrative and are used to help understand the present invention, and are not intended to specifically limit the shapes and proportional dimensions of the various components of the present invention. Those skilled in the art can select various possible shapes and proportional dimensions to implement the present invention according to specific circumstances under the guidance of the present invention.

[0028] Figure 1 This is a structural schematic diagram of an embodiment of the gas-solid reaction device of the present invention.

[0029] Reference numerals in the above drawings:

[0030] 1. Riser reaction assembly; 11. First expansion structure; 111. First annular distributor; 112. Diffuser distributor; 12. Pre-reaction section; 120. First gas-phase feed hole group; 121. First gas-phase feed hole; 13. First reduction structure; 14. Riser section; 140. Second gas-phase feed hole group; 141. Second gas-phase feed hole;

[0031] 2. Bend pipe;

[0032] 3. Downer bed reaction assembly; 31. Second diameter expansion structure; 32. Downer bed; 320. Third gas phase feed hole group; 321. Third gas phase feed hole; 33. Second diameter reduction structure;

[0033] 4. Separation circulation component; 41. Axial flow gas-solid separator; 42. Separation pipeline; 421. Purified gas discharge pipe; 422. Collected particle discharge pipe; 43. Storage bed; 44. Filter component; 45. Unloading valve; 46. Second ring pipe distributor; 47. Discharge valve; 48. Fluidizing gas inlet; 49. Connecting pipeline. DETAILED DESCRIPTION

[0034] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0035] Implementation Method 1

[0036] Please refer to Figure 1As shown, an embodiment of the present invention provides a gas-solid reaction device, which includes at least a riser reaction assembly 1, a downer reaction assembly 3 and a separation circulation assembly 4. The riser reaction assembly 1 includes a pre-reaction section 12 and a riser section 14 connected to the outlet of the pre-reaction section 12; the downer reaction assembly 3 includes a downer 32, the downer 32 and the riser section 14 are arranged side by side, and the inlet of the downer 32 is connected to the outlet of the riser section 14 through a bend 2; the separation circulation assembly 4 includes an axial A flow gas-solid separator 41, a storage companion bed 43, and a connecting pipeline 49 connecting the outlet of the storage companion bed 43 and the inlet of the pre-reaction section 12. The connecting pipeline 49 is provided with a fluidizing gas inlet 48. The inlet of the axial flow gas-solid separator 41 is connected to the outlet of the downer 32. The gas phase outlet of the axial flow gas-solid separator 41 is connected to the gas phase area of ​​the storage companion bed 43 through the purified gas discharge pipe 421. The solid phase outlet of the axial flow gas-solid separator 41 is connected to the storage area of ​​the storage companion bed 43 through the captured particle discharge pipe 422.

[0037] On the whole, the gas-solid reaction device of the present invention is suitable for ultrafine particles. By providing a riser reaction assembly 1 and a down-bed reaction assembly 3, the gas-solid reaction of ultrafine particles mainly occurs in the dilute phase bed section, effectively enhancing the contact and mixing efficiency between the gas and the solid, and avoiding the common problems of insufficient gas-solid contact, adhesion between particles, and heat exchange dead zones in the dense phase bed section. In addition, an axial flow gas-solid separator 41 is configured at the end of the down-bed 32 to achieve rapid and efficient gas-solid separation, reduce the burden of the subsequent filtration assembly 44, and optimize the stable operation cycle of the entire device. By making the riser reaction assembly 1, the down-bed reaction assembly 3, and the separation circulation assembly 4 form a circulation pipeline, the total reaction time of the solid phase can be adjusted as needed, thereby enhancing the flexibility of operation. The gas-solid reaction device also has the advantages of saving space and having great operational flexibility, which improves the reaction efficiency and system reliability as a whole.

[0038] In the embodiment of the present invention, the designer can adjust the specific structure of the axial flow gas-solid separator 41 according to the needs of use, and no specific restrictions are imposed here. Preferably, the axial flow gas-solid separator 41 is arranged at the end of the down-flow bed 32, and the axial flow gas-solid separator 41 includes at least two forms: one is composed of structures such as guide blades, cone sections, and air risers; the other is composed of a swirl head outlet. The down-flow bed 32 is connected to the axial flow gas-solid separator 41 through the second reducing structure 33, and the axial flow gas-solid separator 41 is connected to the storage companion bed 43 through a separation pipeline 42. Among them, the separation pipeline 42 is composed of a purified gas exhaust pipe 421 and a captured particle exhaust pipe 422.

[0039] In this embodiment, the multiphase fluid reaching the end of the down-flow bed 32 is rapidly separated under the combined action of inertial separation and centrifugal separation of the axial flow gas-solid separator 41. Compared with the traditional cyclone separator, the axial flow gas-solid separator 41 has a higher particle size efficiency for particles with a particle size of less than 20 μm, can effectively enhance the overall separation efficiency, and reduce the burden on the subsequent gas-solid separation system.

[0040] Specifically, such as Figure 1 As shown, along the transport direction of the ultrafine particles in the down bed 32, an axial flow gas-solid separator 41 is provided at the end of the down bed 32, and the purified gas discharge pipe 421 and the captured particle discharge pipe 422 in the separation pipeline 42 are both provided on the axial flow gas-solid separator 41, providing a circulation loop for the multiphase fluid.

[0041] In an embodiment of the present invention, the radial dimension of the pre-reaction section 12 is greater than the radial dimension of the lifting pipe section 14, and a first diameter reducing structure 13 is provided between the pre-reaction section 12 and the lifting pipe section 14; and / or, the radial dimension of the pre-reaction section 12 is greater than the radial dimension of the connecting pipeline 49, and a first diameter expanding structure 11 is provided between the pre-reaction section 12 and the connecting pipeline 49; and / or, the radial dimension of the down-bend 32 is greater than the radial dimension of the elbow 2, and a second diameter expanding structure 31 is provided between the down-bend 32 and the elbow 2; and / or, the radial dimension of the down-bend 32 is greater than the radial dimension of the axial flow gas-solid separator 41, and a second diameter reducing structure 33 is provided between the down-bend 32 and the axial flow gas-solid separator 41.

[0042] Preferably, the radial dimension of the pre-reaction section 12 is greater than the radial dimension of the lifting pipe section 14, and a first diameter reducing structure 13 is provided between the pre-reaction section 12 and the lifting pipe section 14; and, the radial dimension of the pre-reaction section 12 is greater than the radial dimension of the connecting pipeline 49, and a first diameter expanding structure 11 is provided between the pre-reaction section 12 and the connecting pipeline 49; and, the radial dimension of the down-down bed 32 is greater than the radial dimension of the elbow 2, and a second diameter expanding structure 31 is provided between the down-down bed 32 and the elbow 2; and, the radial dimension of the down-down bed 32 is greater than the radial dimension of the axial flow gas-solid separator 41, and a second diameter reducing structure 33 is provided between the down-down bed 32 and the axial flow gas-solid separator 41.

[0043] By respectively arranging the first diameter-expanding structure 11 and the first diameter-reducing structure 13 at both ends of the pre-reaction section 12, the pre-reaction section 12 is designed to expand in diameter, which is beneficial to reducing the air flow velocity in the pre-reaction section 12, thereby increasing the contact time between the gas and the ultrafine particles, thereby improving the reaction efficiency.

[0044] In addition, by arranging a second diameter-expanding structure 31 and a second diameter-reducing structure 33 at both ends of the down-bend 32, the down-bend 32 is designed to expand in diameter, which not only significantly reduces the agglomeration of ultrafine particles during the flow process, but also moderately increases the solid phase concentration in the down-bend 32, further improving the gas-solid contact and mixing efficiency.

[0045] Designers can adjust the shapes and structures of the first diameter-expanding structure 11 , the first diameter-reducing structure 13 , the second diameter-expanding structure 31 and the second diameter-reducing structure 33 according to usage requirements, and no specific limitation is imposed herein.

[0046] Preferably, the first diameter-expanding structure 11, the first diameter-reducing structure 13, the second diameter-expanding structure 31, and the second diameter-reducing structure 33 are arranged in a substantially funnel shape. The ratio of the diameters of the upstream end to the downstream end of the first diameter-reducing structure 13 is 1.2 to 3. The ratio of the diameters of the upstream end to the downstream end of the second diameter-reducing structure 33 is 0.6 to 9.

[0047] In an embodiment of the present invention, the gas-solid reaction device also includes at least one diffusion distributor 112 arranged in the pre-reaction section 12, the outlet of the connecting pipeline 49 is connected to the diffusion distributor 112, and the diffusion distributor 112 includes an outlet surface provided with diffusion holes, and the porosity of the outlet surface is 5% to 50%.

[0048] By arranging at least one diffusion distributor 112 in the pre-reaction section 12 and connecting the outlet of the connecting pipeline 49 to the diffusion distributor 112 , the gas and ultrafine particles can be more evenly distributed when entering the pre-reaction section 12 .

[0049] In addition, the outlet surface of the diffusion distributor 112 is provided with diffusion holes with an opening rate of 5% to 50%, which helps to further optimize the gas-solid mixing effect, reduce the phenomenon of local over-concentration or over-diluteness, improve the uniformity of the reactants and the reaction efficiency, thereby enhancing the uniformity of gas-solid contact and helping to improve the overall performance and stability of the gas-solid reaction device.

[0050] Designers can adjust the shape, number, and size of the diffusion holes, as well as the porosity of the outlet surface, based on actual use, without specific limitations. For example, the porosity of the outlet surface can be 5%, 15%, 25%, 35%, 50%, or other values.

[0051] In an embodiment of the present invention, the gas-solid reaction device further includes a first loop pipe distributor 111 arranged in the pre-reaction section 12, the first loop pipe distributor 111 is horizontally arranged and placed upstream of the diffusion distributor 112; and / or, the gas-solid reaction device further includes a second loop pipe distributor 46 arranged in the storage companion bed 43, the second loop pipe distributor 46 is horizontally arranged and placed at the bottom of the storage companion bed 43.

[0052] Preferably, the gas-solid reaction device includes a first annular pipe distributor 111 disposed in the pre-reaction section 12 and a second annular pipe distributor 46 disposed in the storage companion bed 43. The second annular pipe distributor 46 in the storage companion bed 43 is entirely lower than the captured particle discharge pipe 422.

[0053] By setting up a first ring tube distributor 111 in the pre-reaction section 12 and arranging it horizontally upstream of the diffusion distributor 112, the initial distribution of gas and ultrafine particles can be further optimized, ensuring that they have been preliminarily and evenly mixed before entering the diffusion distributor 112, thereby helping to improve the gas-solid contact efficiency and reaction uniformity in the subsequent reaction process.

[0054] Furthermore, by providing a second annular pipe distributor 46 in the storage companion bed 43 and arranging it horizontally at the bottom of the storage companion bed 43, the material distribution in the storage companion bed 43 can be effectively improved, and the occurrence of local accumulation or dead zones can be prevented, thereby improving the operating stability and reaction efficiency of the entire device.

[0055] In an embodiment of the present invention, the ratio of the diameter D1 of the pre-reaction section 12 to the diameter D2 of the riser section 14 is 1.2 to 3; and / or the bending radius R of the elbow 2 and the diameter of the elbow 2 are 0.5 to 10; and / or the ratio of the diameter D3 of the downer 32 to the diameter D1 of the pre-reaction section 12 is 0.5 to 3.

[0056] Preferably, the ratio of the diameter D1 of the pre-reaction section 12 to the diameter D2 of the riser section 14 is 1.2 to 3; and the bending radius R of the elbow 2 and the diameter of the elbow 2 are 0.5 to 10; and the ratio of the diameter D3 of the downer 32 to the diameter D1 of the pre-reaction section 12 is 0.5 to 3.

[0057] By setting the diameter D1 of the pre-reaction section 12 to 1.2 to 3 times the diameter D2 of the riser section 14, and setting the diameter D3 of the downer 32 to 0.5 to 3 times the diameter D1 of the pre-reaction section 12, gas-solid mixing and flow characteristics can be optimized, thereby improving reaction efficiency. The diameter D2 of the riser section 14 can be the same as, or substantially the same as, the diameter of the elbow 2.

[0058] Furthermore, the ratio of the bend radius R of bend 2 to its diameter is between 0.5 and 10. This design effectively reduces pressure drop in the bend 2 region, minimizing energy loss and ensuring smoother passage of gas and ultrafine particles through the bend 2. It also avoids issues such as increased flow resistance and particle deposition caused by excessive curvature of bend 2. Designers can adjust the specific diameter ratio based on specific needs; no specific numerical limit is imposed here.

[0059] In the embodiments of the present application, at least one first gas phase feeding hole group 120 is arranged on the pre-reaction section 12 along the circumferential direction of the pre-reaction section 12; and / or, at least one second gas phase feeding hole group 140 is arranged on the riser section 14 along the circumferential direction of the riser section 14; and / or, at least one third gas phase feeding hole group 320 is arranged on the downer 32 along the circumferential direction of the downer 32.

[0060] Preferably, at least one first gas phase feeding hole group 120 is arranged on the pre-reaction section 12, at least one second gas phase feeding hole group 140 is arranged on the riser section 14, and at least one third gas phase feeding hole group 320 is arranged on the downer 32. The at least one first gas phase feeding hole group 120, the at least one second gas phase feeding hole group 140, and the at least one third gas phase feeding hole group 320 are arranged along the height direction.

[0061] More preferably, a plurality of first gas phase feeding hole groups 120 are arranged on the pre-reaction section 12, a plurality of second gas phase feeding hole groups 140 are arranged on the riser section 14, and a plurality of third gas phase feeding hole groups 320 are arranged on the downer 32.

[0062] For example, the first gas phase feeding hole group 120 is arranged in 1 to 16 rows, the second gas phase feeding hole group 140 is arranged in 1 to 16 rows, and the third gas phase feeding hole group 320 is arranged in 1 to 16 rows.

[0063] In the embodiments of the present application, the specific structure, the number, and the arrangement position of the first gas phase feeding hole group 120 can be adjusted by the designer according to the use requirement, which is not specifically limited herein.

[0064] Preferably, the first gas phase feeding hole group 120 comprises at least one first gas phase feeding hole arranged on the pre-reaction section 12 along the height direction, and a first gas phase nozzle arranged on each first gas phase feeding hole 121, and the included angle a between the incident direction of the first gas phase nozzle and the movement direction of the multiphase fluid in the pre-reaction section 12 is 10° to 170°.

[0065] More preferably, the first gas phase feeding hole group 120 comprises a plurality of first gas phase feeding holes 121 arranged on the pre-reaction section 12 along the height direction. For example, each first gas phase feeding hole group 120 has 2 to 10 first gas phase feeding holes 121.

[0066] In the embodiments of the present application, the specific structure, the number, and the arrangement position of the second gas phase feeding hole group 140 can be adjusted by the designer according to the use requirement, which is not specifically limited herein.

[0067] Preferably, the second gas phase feeding hole group 140 comprises at least one second gas phase feeding hole 141 arranged on the riser section 14 along the height direction, and a second gas phase nozzle arranged on each second gas phase feeding hole 141, and the included angle between the incident direction of the second gas phase nozzle and the movement direction of the multiphase fluid in the riser section 14 is 10° to 170°.

[0068] More preferably, the second gas-phase feed hole group 140 includes a plurality of second gas-phase feed holes 141 arranged along the height direction on the riser section 14. For example, each row of the second gas-phase feed hole group 140 has 2 to 10 second gas-phase feed holes 141.

[0069] Designers can adjust the specific structure, number and arrangement position of the third gas-phase feed hole group 320 according to usage requirements, and no specific restrictions are imposed here.

[0070] Preferably, the third gas-phase feed hole group 320 includes at least one third gas-phase feed hole 321 arranged on the down-bed 32 along the height direction, and a third gas-phase nozzle arranged on each third gas-phase feed hole 321, and the angle between the incident direction of the third gas-phase nozzle and the movement direction of the multiphase fluid in the down-bed 32 is 10° to 170°.

[0071] More preferably, the third gas-phase feed hole group 320 includes a plurality of third gas-phase feed holes 321 arranged along the height direction on the downer 32. For example, each column of the third gas-phase feed hole group 320 has 2 to 10 third gas-phase feed holes 321.

[0072] By respectively arranging at least one row of gas-phase feed hole groups on the pre-reaction section 12, the riser section 14 and the down-bed 32, the fluidizing gas and the raw gas can be supplemented during the reaction process, and multi-point gas intake can be achieved through the gas-phase feed hole groups, which helps to improve the contact opportunity and mixing uniformity of the gas and ultrafine particles, and increases the operational flexibility of the raw gas feed amount in the riser reaction assembly 1 and the down-bed reaction assembly 3.

[0073] Furthermore, by providing gas-phase feed hole groups, the gas distribution within each zone can be better controlled, ensuring a more even dispersion of reactants throughout the reactor, thereby improving reaction efficiency and product quality. Furthermore, multi-point gas inlet reduces the occurrence of localized over-concentration or over-dilute gas, avoiding incomplete reactions or increased side reactions caused by uneven gas distribution, thereby enhancing the system's operational stability and overall performance.

[0074] In an embodiment of the present invention, the gas-solid reaction device further includes a dust-containing gas filtering assembly 44 disposed on the top of the storage companion bed 43 .

[0075] By installing a dust-laden gas filter assembly 44 atop the storage companion bed 43, dust and other particulate matter generated during the reaction process can be effectively removed, ensuring cleaner exhaust gas. This reduces environmental pollution and improves the operational stability of the entire system, preventing equipment failure or performance degradation caused by dust accumulation. Furthermore, clean exhaust gas helps meet environmental protection requirements and improves the overall operational efficiency and sustainability of the device.

[0076] The specific structure of the dust-laden gas filter assembly 44 can be adjusted by the designer according to the actual use requirements and is not specifically limited here. For example, the dust-laden gas filter assembly 44 can be a dust removal device such as a bag filter, an electrostatic precipitator, or a cyclone separator, or the dust-laden gas filter assembly 44 can also have other structures.

[0077] In an embodiment of the present invention, the gas-solid reaction device further includes a discharge valve 45 provided at the bottom of the storage companion bed 43 , and a discharge valve 47 provided at the outlet of the storage companion bed 43 .

[0078] By arranging a discharge valve 45 at the bottom of the storage companion bed 43 and a discharge valve 47 at the outlet of the storage companion bed 43 , precise control of the flow of solid materials can be achieved.

[0079] The discharge valve 45 is located at the bottom of the storage bed 43, which helps to discharge the solid materials accumulated in the gas-solid reaction device regularly or as needed, ensuring that the operation efficiency of the gas-solid reaction device will not be affected by the accumulation of materials in the storage bed 43.

[0080] The discharge valve 47 can control the flow of materials from the storage bed 43 to the subsequent processing steps to ensure the continuity and stability of material transportation. The designer can adjust the specific models of the discharge valve 45 and the discharge valve 47 according to the needs of use, and no specific restrictions are made here.

[0081] Implementation Method 2

[0082] An embodiment of the present invention provides a gas-solid reaction method, which is implemented using the gas-solid reaction device in the first embodiment. The gas-solid reaction method includes the following steps:

[0083] Step S1000: close the discharge valve 45 and start the gas phase supply of the second annular pipe distributor 46 to make the ultrafine particles in the storage bed 43 flow;

[0084] Step S2000: Open the discharge valve 47 and simultaneously open the fluidizing gas inlet 48 to introduce fluidizing gas and feed gas into the connecting pipeline 49 to transport the ultrafine particles, and maintain the superficial gas velocity in the riser reaction assembly 1 within the entrained gas range;

[0085] Step S3000: Open the first loop distributor 111 to introduce supplementary fluidizing gas into the pre-reaction section 12 to avoid formation of a dead zone at the bottom of the pre-reaction section 12;

[0086] Step S4000: During the reaction of the ultrafine particles, fluidizing gas and feed gas are introduced into the riser reaction assembly 1 and / or the downer reaction assembly 3 to maintain the feed gas concentration in the reaction assembly; wherein the feed gas injection velocity in the riser reaction assembly 1 and / or the downer reaction assembly 3 is 10 m / s to 100 m / s;

[0087] Step S5000: After the ultrafine particles react in the riser reaction assembly 1 and the downer reaction assembly 3, the multiphase fluid output from the downer 32 is separated by the axial flow gas-solid separator 41. The separated ultrafine particles are returned to the storage companion bed 43 for continued circulation. The separated gas phase fluid is returned to the storage companion bed 43 and discharged after filtration.

[0088] Step S6000: After the ultrafine particles complete the reaction cycle, the discharge valve 47 is closed to stop the cycle, and the discharge valve 45 is opened to discharge the ultrafine particles.

[0089] The gas-solid reaction method of the present invention regulates the gas flow rate at the fluidizing gas inlet 48 to maintain the superficial gas velocity within the riser reaction assembly 1 within the entrainment velocity range. Simultaneously, feed gas is replenished via gas nozzles within the riser reaction assembly 1 and the downer reaction assembly 3, maintaining the feed gas concentration within the reaction assembly within the desired range. Furthermore, an axial flow gas-solid separator 41 achieves efficient gas-solid separation of the multiphase fluid completing the cycle. Furthermore, the circulation and extraction of ultrafine particles are controlled by a feed valve 47 and a discharge valve 45, enabling flexible operation of the target product production process.

[0090] After the ultrafine particles have completed a single circulation process, the axial flow gas-solid separator 41 removes most of the ultrafine particles from the multiphase fluid and directs them back into the storage companion bed 43 via the particle collection discharge pipe 422. The gaseous fluid carrying a small amount of unseparated particles is directed back into the center of the storage companion bed 43 via the purified gas discharge pipe 421. Before discharge, the gaseous phase in the storage companion bed 43 is further separated by passing through the dust-laden gas filter assembly 44, and the filter element of the dust-laden gas filter assembly 44 is regularly backflushed. The ultrafine particles returned to the storage companion bed 43 continue to circulate.

[0091] In this embodiment, the raw material gas is a gas-solid high-efficiency reaction gas, and the fluidizing gas is a protective gas such as an inert gas, which is not limited in the present invention.

[0092] In this embodiment, when a rapid gas-solid reaction is carried out in the riser reaction assembly 1 and the down-bed reaction assembly 3, the ratio of the raw gas and the fluidizing gas entering the reaction assembly through the gas phase nozzle is higher than the ratio of the raw gas and the fluidizing gas introduced through the fluidizing gas inlet 48, so as to ensure that the raw gas concentration in the reaction assembly is maintained at an ideal level.

[0093] In an embodiment of the present invention, by providing a pre-reaction section 12 with a diameter ratio of 1.2 to 3, a riser section 14, and a downer 32 with a diameter 0.5 to 3 times the diameter D1 of the pre-reaction section 12, it is convenient to automatically adjust the superficial gas velocity in the riser reaction assembly 1 and the downer reaction assembly 3, thereby realizing the circulation and transportation of ultrafine particles in the reaction assembly.

[0094] In an embodiment of the present invention, the separated gas phase fluid is transported back to the storage companion bed 43 and discharged after filtration, specifically comprising the following steps:

[0095] Step S5100: Remove a small amount of solid phase entrained in the gas phase fluid through the dust-laden gas filter assembly 44 and discharge the gas filtered by the dust-laden gas filter assembly 44. During use, the dust-laden gas filter assembly 44 can be back-flushed regularly.

[0096] In an embodiment of the present invention, the steps of introducing fluidizing gas and feed gas into the riser reaction assembly 1 and / or the downer reaction assembly 3 to maintain the feed gas concentration in the reaction assembly specifically include the following steps:

[0097] Step S4100: Fluidizing gas and raw gas are introduced into the pre-reaction section 12 through the first gas-phase feed hole group 120 to maintain the raw gas concentration in the reaction assembly; and / or, fluidizing gas and raw gas are introduced into the riser section 14 through the second gas-phase feed hole group 140 to maintain the raw gas concentration in the reaction assembly; and / or, fluidizing gas and raw gas are introduced into the downward bed 32 through the third gas-phase feed hole group 320 to maintain the raw gas concentration in the reaction assembly.

[0098] Designers can adjust the opening and closing states of each first gas-phase feed hole group 120 , each second gas-phase feed hole group 140 , and each third gas-phase feed hole group 320 according to usage needs, and no specific limitation is imposed here.

[0099] All articles and references disclosed, including patent applications and publications, are incorporated herein by reference for all purposes. The term "essentially consisting of..." describing a combination should include the identified elements, ingredients, parts or steps and other elements, ingredients, parts or steps that do not substantially affect the basic novel features of the combination. The use of the terms "comprising" or "including" to describe the combination of elements, ingredients, parts or steps herein also contemplates an embodiment that is essentially composed of these elements, ingredients, parts or steps. By using the term "may", it is intended to illustrate that any attribute described that "may" include is optional. Multiple elements, ingredients, parts or steps can be provided by a single integrated element, ingredient, part or step. Alternatively, a single integrated element, ingredient, part or step can be divided into separate multiple elements, ingredients, parts or steps. The disclosure "one" or "an" used to describe an element, ingredient, part or step is not intended to exclude other elements, ingredients, parts or steps.

[0100] Each embodiment in this specification is described in a progressive manner, and each embodiment focuses on the differences from other embodiments. The same or similar parts between the embodiments can be referred to each other. The above embodiments are only for illustrating the technical concept and features of the present invention. Their purpose is to enable people familiar with this technology to understand the content of the present invention and implement it accordingly, and they cannot be used to limit the scope of protection of the present invention. Any equivalent changes or modifications made according to the spirit of the present invention should be included in the scope of protection of the present invention.

Claims

1. A gas-solid reaction device, characterized in that: include: A riser reaction assembly, the riser reaction assembly comprising a pre-reaction section and a riser section connected to the outlet of the pre-reaction section; A downer reaction assembly, the downer reaction assembly comprising a downer, the downer and the riser section being arranged side by side, the inlet of the downer being connected to the outlet of the riser via an elbow; A separation circulation assembly, comprising an axial flow gas-solid separator, a storage companion bed, and a connecting pipeline connecting the outlet of the storage companion bed and the inlet of the pre-reaction section, wherein the connecting pipeline is provided with a fluidizing gas inlet, the inlet of the axial flow gas-solid separator is connected to the outlet of the downer, the gas phase outlet of the axial flow gas-solid separator is connected to the gas phase region of the storage companion bed via a purified gas discharge pipe, and the solid phase outlet of the axial flow gas-solid separator is connected to the storage region of the storage companion bed via a captured particle discharge pipe; The radial dimension of the pre-reaction section is larger than the radial dimension of the lifting pipe section, and a first diameter reducing structure is provided between the pre-reaction section and the lifting pipe section; and / or, the radial dimension of the pre-reaction section is larger than the radial dimension of the connecting pipeline, and a first diameter expanding structure is provided between the pre-reaction section and the connecting pipeline; and / or, the radial dimension of the downer is larger than the radial dimension of the elbow, and a second diameter expanding structure is provided between the downer and the elbow; and / or, the radial dimension of the downer is larger than the radial dimension of the axial flow gas-solid separator, and a second diameter reducing structure is provided between the downer and the axial flow gas-solid separator.

2. The gas-solid reaction device according to claim 1, characterized in that: The gas-solid reaction device also includes at least one diffusion distributor arranged in the pre-reaction section, the outlet of the connecting pipeline is connected to the diffusion distributor, and the diffusion distributor includes an outlet surface provided with diffusion holes, and the porosity of the outlet surface is 5% to 50%.

3. The gas-solid reaction device according to claim 2, characterized in that: The gas-solid reaction device further includes a first loop pipe distributor arranged in the pre-reaction section, the first loop pipe distributor is horizontally arranged and placed upstream of the diffusion distributor; and / or, the gas-solid reaction device further includes a second loop pipe distributor arranged in the material storage companion bed, the second loop pipe distributor is horizontally arranged and placed at the bottom of the material storage companion bed.

4. The gas-solid reaction device according to claim 3, characterized in that: The ratio of the diameter of the pre-reaction section to the diameter of the riser section is 1.2 to 3; and / or the bending radius R of the elbow and the diameter of the elbow are 0.5 to 10; and / or the ratio of the diameter of the downer to the diameter of the pre-reaction section is 0.5 to 3.

5. The gas-solid reaction device according to claim 4, characterized in that: Along the circumference of the pre-reaction section, at least one row of first gas-phase feed hole groups is provided on the pre-reaction section; and / or, along the circumference of the riser section, at least one row of second gas-phase feed hole groups is provided on the riser section; and / or, along the circumference of the downer, at least one row of third gas-phase feed hole groups is provided on the downer.

6. The gas-solid reaction device according to claim 5, characterized in that: The first gas-phase feed hole group includes at least one first gas-phase feed hole arranged on the pre-reaction section along the height direction, and a first gas-phase nozzle arranged on each of the first gas-phase feed holes, and the angle between the incident direction of the first gas-phase nozzle and the movement direction of the multiphase fluid in the pre-reaction section is 10° to 170°; and / or, the second gas-phase feed hole group includes at least one second gas-phase feed hole arranged on the riser section along the height direction, and a second gas-phase nozzle arranged on each of the second gas-phase feed holes, and the angle between the incident direction of the second gas-phase nozzle and the movement direction of the multiphase fluid in the riser section is 10° to 170°; and / or, the third gas-phase feed hole group includes at least one third gas-phase feed hole arranged on the down-bed along the height direction, and a third gas-phase nozzle arranged on each of the third gas-phase feed holes, and the angle between the incident direction of the third gas-phase nozzle and the movement direction of the multiphase fluid in the down-bed is 10° to 170°.

7. The gas-solid reaction device according to claim 5, characterized in that: The gas-solid reaction device further comprises a dust-containing gas filtering assembly arranged on the top of the storage bed.

8. The gas-solid reaction device according to claim 7, characterized in that: The gas-solid reaction device further includes a discharge valve arranged at the bottom of the material storage companion bed, and a feed valve arranged at the outlet of the material storage companion bed.

9. A gas-solid reaction method, characterized in that: The gas-solid reaction method is implemented by using the gas-solid reaction device according to claim 8, and comprises the following steps: Close the discharge valve and open the gas phase supply of the second ring pipe distributor to make the ultrafine particles in the storage bed in a flowing state; Open the discharge valve and the fluidizing gas inlet at the same time to introduce fluidizing gas and feed gas into the connecting pipeline to transport ultrafine particles, and maintain the superficial gas velocity in the riser reaction assembly within the entrained gas range; Opening the first loop distributor to introduce supplementary fluidizing gas into the pre-reaction section to avoid formation of a dead zone at the bottom of the pre-reaction section; During the reaction of the ultrafine particles, fluidizing gas and feed gas are introduced into the riser reaction assembly and / or the downer reaction assembly to maintain the feed gas concentration in the reaction assembly; wherein the feed gas injection velocity in the riser reaction assembly and / or the downer reaction assembly is 10 m / s to 100 m / s; After the ultrafine particles have reacted in the riser reaction assembly and the downer reaction assembly in sequence, the multiphase fluid output from the downer is separated by an axial flow gas-solid separator, the separated ultrafine particles are transported back to the storage companion bed to continue circulating, and the separated gas phase fluid is transported back to the storage companion bed and discharged after being filtered. When the ultrafine particles complete the reaction cycle, the discharge valve is closed to stop the cycle, and the discharge valve is opened to discharge the ultrafine particles.

Images